Analysis of trace microcystins in vegetables using matrix solid-phase dispersion followed by high performance liquid chromatography triple-quadrupole mass spectrometry detection

• Published in: Talanta (Oxford) Vol. 173; pp. 101 - 106
• Main Authors: Qian, Zong-Yao, Li, Zhi-Gang, Ma, Jian, Gong, Ting-ting, Xian, Qi-Ming
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 01.10.2017
• Subjects: Chromatography, High Pressure Liquid; color; cucumbers; detection limit; Determination; Food Analysis - methods; Food Contamination - analysis; high performance liquid chromatography; Lake Taihu; LC-MS/MS; Limit of Detection; Linear Models; Mass Drug Administration; mass spectrometry; Microcystin; microcystins; Microcystins - analysis; Microcystins - isolation & purification; monitoring; MSPD; solid phase extraction; Solid Phase Extraction - methods; solvents; Spinacia; tomatoes; Vegetable; Vegetables - chemistry; Microcystin; LC-MS/MS; Determination; MSPD; Vegetable; Lake Taihu
• DOI: 10.1016/j.talanta.2017.05.079
• ISSN: 0039-9140; 1873-3573

A selective and sensitive method for the simultaneous determination of five common microcystins (MC-LR, -RR, -YR, -LW, -LF) in various vegetables was established using Matrix Solid-Phase Dispersion (MSPD) followed by high performance liquid chromatography-mass spectrometry detection. To optimize the pretreatment procedure for extracting the microcystins from three vegetable matrices (tomato, cucumber and spinacia, which represented different colors), Box-Behnken design was employed to optimize the main factors affecting the extraction efficiency, including sample/dispersant mass ratio, as well as the proportion mixture dispersant and the volumes of solvent. Based on the optimum conditions, the intra-day and inter-day variability for each microcystins in all vegetable samples were less than 8.6%, with the recoveries ranging from 71.9% to 96.5%. The limits of detection and quantitation of the method were 13.0μg/kg (dw) and 43.0μg/kg (dw), respectively. The established method was successfully applied to the analysis of MCs in vegetable samples which were collected by Lake Taihu. The procedure promising to be relative small sample size and short pretreatment time for the assay that can be used for monitoring MCs concentrations in vegetables. [Display omitted] •A MSPD-HPLC-MS/MS method was first proposed for microcystins residue detection.•Key factors affecting the extraction were evaluated by Box-Behnken Design.•The proposed method exhibits good reproducibility and high sensitivity.